WO2014142019A1 - Poudre pour pulvérisation thermique, revêtement appliqué pour pulvérisation thermique, et procédé de formation d'un revêtement appliqué par pulvérisation thermique - Google Patents

Poudre pour pulvérisation thermique, revêtement appliqué pour pulvérisation thermique, et procédé de formation d'un revêtement appliqué par pulvérisation thermique Download PDF

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Publication number
WO2014142019A1
WO2014142019A1 PCT/JP2014/055936 JP2014055936W WO2014142019A1 WO 2014142019 A1 WO2014142019 A1 WO 2014142019A1 JP 2014055936 W JP2014055936 W JP 2014055936W WO 2014142019 A1 WO2014142019 A1 WO 2014142019A1
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Prior art keywords
powder
thermal
thermal spraying
ceramic particles
thermal spray
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PCT/JP2014/055936
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English (en)
Japanese (ja)
Inventor
順也 北村
和人 佐藤
一志 都築
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株式会社 フジミインコーポレーテッド
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Priority to KR1020157027729A priority Critical patent/KR102164024B1/ko
Priority to US14/774,061 priority patent/US9682892B2/en
Priority to JP2015505438A priority patent/JP6262716B2/ja
Publication of WO2014142019A1 publication Critical patent/WO2014142019A1/fr

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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/444—Halide containing anions, e.g. bromide, iodate, chlorite
    • C04B2235/445—Fluoride containing anions, e.g. fluosilicate
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5296—Constituents or additives characterised by their shapes with a defined aspect ratio, e.g. indicating sphericity
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron

Definitions

  • the present invention relates to a thermal spraying powder containing ceramic particles, a thermal spray coating formed using the thermal spraying powder, and a method for forming the thermal spray coating.
  • Ceramic spray coating is used in various applications depending on the characteristics of the constituent ceramics.
  • an aluminum oxide sprayed coating is used as a protective coating for various members because aluminum oxide exhibits high electrical insulation, wear resistance, and corrosion resistance.
  • the yttrium oxide sprayed coating is used as a protective coating for members in semiconductor device manufacturing apparatuses because yttrium oxide exhibits high plasma erosion resistance (see, for example, Patent Documents 1 and 2).
  • the ceramic thermal spray coating may be inferior in mechanical, electrical or chemical properties compared to a ceramic sintered bulk.
  • an aluminum oxide sprayed coating is inferior in electrical insulation, wear resistance, or corrosion resistance as compared with an aluminum oxide sintered bulk body.
  • the yttrium oxide sprayed coating is inferior in plasma erosion resistance as compared with a yttrium oxide bulk bulk.
  • Ceramic particles having a small particle diameter it is effective to use ceramic particles having a small particle diameter in order to form a ceramic sprayed coating having characteristics close to those of a sintered ceramic bulk body. For example, by spraying ceramic particles having an average particle size of 10 ⁇ m or less, a dense ceramic sprayed coating having a low porosity may be obtained. However, ceramic particles having a small particle size tend to be inferior in fluidity.
  • Carr's fluidity index is used to design a thermal spraying powder having a required fluidity. Carr's fluidity index is determined from the angle of repose, the degree of compression, the spatula angle, and the degree of aggregation (or uniformity). However, in the case of ceramic particles having an average particle size of 10 ⁇ m or less, the correlation between Carr's fluidity index and actual fluidity is poor, and it is difficult to design to have the required fluidity. The inventors of the invention have found.
  • an object of the present invention is to provide a thermal spraying powder containing ceramic particles designed to have a required fluidity. Another object of the present invention is to provide a thermal spray coating formed using the thermal spray powder and a method for forming the thermal spray coating.
  • a thermal spraying powder containing ceramic particles having an average particle diameter of 1 ⁇ m or more and 20 ⁇ m or less, wherein the ceramic particles are measured using a powder rheometer.
  • the fluidity index value FF is 3 or more.
  • the fluidity index value FF is the maximum principal stress and uniaxial collapse stress of the ceramic particles when a shearing force of 9 kPa is applied to the ceramic particles at normal temperature and humidity.
  • the thermal spraying powder is obtained by measuring the maximum principal stress and dividing the measured value of the maximum principal stress by the measured value of the uniaxial collapse stress.
  • the average fractal dimension value of the ceramic particles is preferably 1.05 or more and 1.7 or less.
  • the ceramic particles may be coated with a polymer. Alternatively, nanoparticles may be attached to the surface of the ceramic particles.
  • the ceramic particles may contain 40% by mass or less of particles having a particle diameter of 20 ⁇ m or more and 50 ⁇ m or less.
  • thermo spray coating obtained by thermal spraying the thermal spraying powder according to the above aspect is provided.
  • thermo spray coating by forming a thermal spray coating by performing high-speed flame spraying or plasma spraying on the thermal spraying powder according to the above-described aspect.
  • the thermal spraying powder may be supplied to the thermal spraying apparatus by an axial feed method.
  • the thermal spraying powder may be supplied to the thermal spraying apparatus by using two feeders so that the fluctuation cycles of the supply amounts of the thermal spraying powders from both feeders are opposite to each other.
  • the thermal spraying powder may be sent out from a feeder, temporarily stored in a tank immediately before the thermal spraying apparatus, and the thermal spraying powder in the tank may be supplied to the thermal spraying apparatus using natural fall.
  • the thermal spraying powder is preferably heated to a temperature of 110% or more of the melting point of the ceramic particles during thermal spraying.
  • the thermal spraying powder is used, for example, in an application for forming a thermal spray coating.
  • a thermal spray coating is formed on the base material.
  • the type of the substrate is not particularly limited, such as metal or ceramic.
  • the thermal spraying powder contains ceramic particles.
  • Ceramic particles in thermal spraying powder include yttrium oxide, aluminum oxide, silicon oxide, titanium oxide, zirconium oxide, yttria stabilized zirconium oxide, chromium oxide, zinc oxide, mullite, yttrium aluminum garnet (YAG), cordierite, zircon, etc. It may be made of oxide ceramics.
  • spinel ceramics scandium (Sc), yttrium (Y), lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), promethium (Pm), samarium (Sm), europium (Eu) , Oxides containing rare earth elements such as gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), lutetium (Lu) Particles made of composite oxide ceramics including ceramics, aluminum (Al), silicon (Si), manganese (Mn), zinc (Zn) and the like may be used. Or the particle
  • the thermal spraying powder may contain components other than ceramic particles, but the content of components other than ceramic particles is preferably as small as possible. Preferably, 100% of the thermal spraying powder is constituted by ceramic particles.
  • the average particle diameter of the ceramic particles in the thermal spraying powder is preferably 1 ⁇ m or more, more preferably 2 ⁇ m or more. In this case, the fluidity of the thermal spraying powder is improved.
  • the average particle size of the ceramic particles in the thermal spraying powder is preferably 20 ⁇ m or less, more preferably 15 ⁇ m or less, still more preferably 10 ⁇ m or less, and most preferably 8 ⁇ m or less. In this case, it becomes easy to obtain a dense ceramic sprayed coating.
  • the ceramic particles in the thermal spraying powder preferably have a fluidity index value FF of 3 or more measured using a powder rheometer such as FT4 manufactured by Malvern.
  • the flowability index value FF is the largest main value of ceramic particles when a predetermined amount of ceramic particles is put in a container having a diameter of 50 mm, for example, and a shearing force of 9 kPa is applied to the ceramic particles in the container under normal temperature and humidity. The stress and uniaxial collapse stress are measured, and the maximum principal stress measurement value is divided by the uniaxial collapse stress measurement value.
  • the fluidity index value FF does not depend on the size of the container in which the ceramic particles are put and the amount of the ceramic particles put in the container.
  • the ceramic particles are allowed to stand for 0.5 hour or longer in a state of a temperature of 20 ° C. and a humidity of 50% RH before the measurement.
  • a thermal spray coating is produced using a thermal spraying powder containing ceramic particles having a fluidity index value FF of 3 or more, it becomes easy to obtain a dense thermal spray coating.
  • the ceramic particles are coated with a polymer or an organic compound, or nanoparticles are attached to the surface of the ceramic particles, or a silane cup It is effective to add a functional group such as a carbonyl group to the surface of the ceramic particle using a ring agent or the like.
  • the coating of the ceramic particles with the polymer or the organic compound can be performed, for example, by mixing the polymer or the organic compound and the ceramic particles with water or an organic solvent and drying the mixture while dispersing the mixture.
  • the ceramic particles may be coated with the polymer by mixing the ceramic particles and the polymer fine powder in the air.
  • the polymer used here include nonionic polymers such as polyethers such as polyethylene glycol.
  • a cellulose is mentioned as an example of an organic compound.
  • the adhesion of the nanoparticles to the surface of the ceramic particles can be performed, for example, by mixing the ceramic particles and the nanoparticles.
  • the nanoparticles used here include ceramic fine particles and carbon fine particles.
  • the nanoparticles preferably have the same composition as the ceramic particles in the thermal spraying powder.
  • the nanoparticles preferably have an average particle size of 200 nm or less.
  • the average fractal dimension value of the ceramic particles is preferably 1.05 or more, more preferably 1.2 or more.
  • the average fractal dimension value is a value obtained by quantifying the degree of unevenness of the ceramic particle surface, and takes a value of 1 or more and less than 2. The higher the unevenness of the ceramic particle surface, the larger the average fractal dimension value of the ceramic particles.
  • the average fractal dimension value of the ceramic particles is also preferably 1.7 or less, and more preferably 1.6 or less. In this case, it becomes easy to reduce the adverse effect of the irregularities on the surface of the ceramic particles on the fluidity of the ceramic particles.
  • the ceramic particles may include particles having a particle diameter of 20 ⁇ m or more and 50 ⁇ m or less. In this case, it is easy to improve the fluidity of the ceramic particles.
  • the proportion of particles having a particle diameter of 20 ⁇ m or more and 50 ⁇ m or more contained in the ceramic particles is preferably 40% by mass or less.
  • Ceramic particles can be produced, for example, by the Bernoulli method or the melt-pulverization method. Alternatively, it may be produced by a solid phase sintering method such as a sintering-grinding method and a granulation-sintering method.
  • a solid phase sintering method such as a sintering-grinding method and a granulation-sintering method.
  • ceramic particles are produced by melting a raw material powder while dropping it in an oxyhydrogen flame and growing crystals.
  • ceramic particles are produced by melting a raw material powder, cooling and solidifying the powder, and then pulverizing and classifying as necessary.
  • ceramic particles are produced by sintering and pulverizing the raw material powder and then classifying it as necessary.
  • the raw material powder is granulated and sintered, and then crushed, and then classified as necessary to produce ceramic particles.
  • the ceramic particles can be produced by a gas phase synthesis method.
  • single crystal particles can be produced by the flux method.
  • the method of spraying the thermal spraying powder is a high-speed flame spraying method in which the thermal spraying powder is supplied to the center of a high-speed combustion flame jet flow generated by high-pressure oxygen (or air) and fuel and continuously injected at a high speed, for example, high-speed oxygen fuel Thermal spraying (HVOF) may be used, or plasma spraying, for example, atmospheric pressure plasma spraying (APS), in which powder for spraying is supplied to the center of a plasma jet generated by a gas in a plasma state and sprayed. Also good.
  • the fuel used in high-speed flame spraying may be a hydrocarbon gas fuel such as acetylene, ethylene, propane, or propylene, or a liquid fuel such as kerosene or ethanol.
  • the thermal spraying powder of the present invention is sprayed by high-speed flame spraying or plasma spraying, the thermal spraying powder having a small particle diameter can be sprayed with good fluidity, and a dense thermal spray coating can be efficiently formed.
  • the thermal spraying powder is preferably heated to a temperature of 110% or more of the melting point of the ceramic particles during thermal spraying. In this case, it becomes easy to obtain a dense sprayed coating by sufficiently heating the ceramic particles during spraying.
  • the spraying distance that is, the distance from the nozzle tip of the spraying device to the base material is preferably 30 mm or more. In this case, it becomes easy to suppress thermal alteration and thermal deformation of the substrate.
  • the spraying distance is also preferably 200 mm or less. In this case, it becomes easy to obtain a dense sprayed coating by sufficiently heating the ceramic particles during spraying.
  • the thermal spraying powder is supplied to the thermal spraying apparatus by an axial feed method, that is, the thermal spraying powder is supplied in the same direction as the axis of the jet flow generated in the thermal spraying apparatus.
  • the thermal spraying powder of the present invention is supplied to the thermal spraying device by the axial feed method, the ceramic particles in the thermal spraying powder are less likely to adhere in the thermal spraying device because of the good fluidity of the thermal spraying powder, and a dense thermal sprayed coating is formed. It can be formed efficiently.
  • the thermal spraying powder of the present invention is supplied to the thermal spraying apparatus by a two-stroke method, since the thermal spraying powder has good fluidity, a dense thermal sprayed coating can be formed efficiently.
  • a tank for temporarily storing the thermal spraying powder sent from the feeder immediately before the thermal spraying device is provided, and the inside of the tank is used by utilizing natural fall.
  • the thermal spraying powder may be supplied to the thermal spraying apparatus.
  • the supply of the thermal spraying powder to the thermal spraying apparatus is preferably performed via a metal conductive tube, for example.
  • a metal conductive tube When a conductive tube is used, it is difficult for fluctuations to occur in the supply amount of the slurry for thermal spraying by suppressing the generation of static electricity.
  • the inner surface of the conductive tube preferably has a surface roughness Ra of 0.2 ⁇ m or less.
  • the thermal spraying powder has the required fluidity suitable for good supply to the thermal spraying device. sell. That is, it can have sufficient fluidity sufficient to form a sprayed coating.
  • thermo spraying powder capable of satisfactorily forming a ceramic thermal spray coating.
  • the thermal spraying powder may contain two or more kinds of ceramic particles.
  • Thermal spray powders of Examples 1 to 10 and Comparative Examples 1 to 4 made of ceramic particles were prepared. Details of each thermal spraying powder are shown in Table 1.
  • the “type of ceramic particles” column in Table 1 indicates the type of ceramic particles used in each thermal spraying powder.
  • “Al 2 O 3 ” represents aluminum oxide
  • “Y 2 O 3 ” represents yttrium oxide
  • “YSZ” represents yttria-stabilized zirconium oxide
  • (La—Yb—Al—Si—) “Zn) O” represents a double oxide ceramic containing lanthanum, ytterbium, aluminum, silicon and zinc
  • (La—Al—Si—Ca—Na—PFB) O” represents lanthanum, aluminum
  • the “average particle size of ceramic particles” column shows the average particle size of ceramic particles used in each thermal spraying powder.
  • the average particle diameter was calculated from the specific surface area of the ceramic particles measured using a specific surface area measuring device “Flow SorbII 2300” manufactured by Micromeritics.
  • the “average fractal dimension value of ceramic particles” column shows the results of measuring the average fractal dimension value of ceramic particles used in each thermal spraying powder. Specifically, the measurement of the average fractal dimension value is performed by measuring the secondary electrons by means of a scanning electron microscope for five particles having an average particle size within ⁇ 3 ⁇ m among the ceramic particles in each thermal spraying powder. Based on the image (magnification 1000 to 2000 times), it was performed by the divider method using the image analysis software Image-Pro Plus of Nippon Roper Co., Ltd.
  • Al 2 O 3 nanoparticles adhering in the “special notes” column of Table 1 indicates that aluminum oxide nanoparticles having an average particle size of 0.1 ⁇ m are adhering to the surface of the ceramic particles, It represents that the content of aluminum oxide nanoparticles is 0.5% by mass.
  • Y 2 O 3 nanoparticles are adhered means that yttrium oxide nanoparticles having an average particle diameter of 0.1 ⁇ m are adhered to the surface of the ceramic particles, and the content of yttrium oxide nanoparticles in the thermal spraying powder is 0. This represents 5% by mass.
  • YSZ nanoparticles are attached means that yttria-stabilized zirconium oxide nanoparticles with an average particle size of 0.1 ⁇ m are attached to the surface of ceramic particles, and the content of yttria-stabilized zirconium oxide nanoparticles in the thermal spraying powder Represents 0.5 mass%.
  • Gram-sintering indicates that the ceramic particles are produced by the granulation-sintering method.
  • Coating with PEG means that the ceramic particles are coated with polyethylene glycol.
  • Constaining Al 2 O 3 coarse particles means that aluminum oxide coarse particles having a particle diameter of 30 ⁇ m are mixed with ceramic particles, and the content of the aluminum oxide coarse particles in the thermal spraying powder is 20% by mass.
  • the column “flowability index value FF” in Table 1 shows the result of measuring the flowability index value FF of the ceramic particles used in each thermal spraying powder using a powder rheometer.
  • the column “Filmability No. 1” in Table 1 shows the results of evaluating whether or not a thermal spray coating could be obtained when each thermal spray powder was subjected to atmospheric pressure plasma spraying under the conditions shown in Table 2. . “ ⁇ (good)” in the same column indicates that the thickness of the sprayed coating formed per pass is 3 ⁇ m or more, and “x (bad)” indicates that it is less than 3 ⁇ m. To express. Note that one pass refers to a single spraying operation performed by the spraying device (spraying gun) along the operation direction of the spraying device or the object to be sprayed (base material).
  • Table 1 shows the result of evaluating the porosity of the thermal spray coating obtained by atmospheric pressure plasma spraying each thermal spray powder under the conditions described in Table 2.
  • the porosity was measured as follows. That is, after the cross section of the sprayed coating was resin-filled and polished, a cross-sectional image thereof was taken using a digital microscope VC-7700 manufactured by OMRON Corporation. And the pore part in a cross-sectional image was specified by the image analysis using image analysis software ImagePro made from Nippon Roper Co., Ltd., and the ratio of the area occupied in the cross-sectional image was obtained. “ ⁇ (good)” in the “Coating Properties No. 1” column indicates that the measured porosity of the sprayed coating was 10% or less, and “x (defect)” indicates that it was more than 10%. "-" Represents untested.
  • the column “Coating properties 2” in Table 1 shows the results of evaluating the porosity of the thermal spray coating obtained by HVOF spraying each thermal spraying powder under the conditions shown in Table 3.
  • “ ⁇ (good)” in the same column indicates that the porosity of the sprayed coating measured by the same method as described above was 10% or less, and “x (bad)” indicates that it was more than 10%.
  • “-" Represents untested.
  • each of the thermal spray coatings obtained from the thermal spraying powders of Examples 1 to 10 had a high density with a porosity of 10% or less.

Abstract

L'invention concerne une poudre pour pulvérisation thermique contenant des particules de céramique ayant un diamètre de particule moyen de 1 µm à 20 µm. L'indice de fluidité (FF) des particules de céramique mesuré à l'aide d'un rhéomètre pour poudres est d'au moins 3. L'indice de fluidité (FF) est obtenu en mesurant la limite d'élasticité non confinée et la contrainte principale majeure de particules de céramique lorsqu'elles sont soumises à une contrainte de cisaillement de 9 kPa à une température et une humidité ambiante, et en divisant la valeur mesurée pour la contrainte principale majeure par la valeur mesurée pour la limite d'élasticité non confinée.
PCT/JP2014/055936 2013-03-13 2014-03-07 Poudre pour pulvérisation thermique, revêtement appliqué pour pulvérisation thermique, et procédé de formation d'un revêtement appliqué par pulvérisation thermique WO2014142019A1 (fr)

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US14/774,061 US9682892B2 (en) 2013-03-13 2014-03-07 Powder for thermal spraying, thermal sprayed coating, and method for forming thermal sprayed coating
JP2015505438A JP6262716B2 (ja) 2013-03-13 2014-03-07 溶射用粉末、及び溶射皮膜の形成方法

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JP2020023410A (ja) * 2018-08-06 2020-02-13 株式会社フジミインコーポレーテッド 粉末材料
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